反応 #455475

反応方程式

5,6-Dichloro-N-hydroxy-3-pyridinecarboximidoyl chloride

triethylamine

1-butyne

→

desired product

収率 90.0%

3-(2,3-Dichloro-5-pyridyl)-5-ethylisoxazole

収率 90.0%

溶媒

ether

ether

反応条件

後処理

1. 1
   その他was bubbled through the reaction mixture
2. 2
   ろ過filtered
3. 3
   その他the filtrate evaporated to dryness under reduced pressure
4. 4
   その他Recrystallisation of the residue from hexane

実験手順

5,6-Dichloro-N-hydroxy-3-pyridinecarboximidoyl chloride (0.85 g, 3.8 mmol) was dissolved with stirring in ether (60 mL) and a solution of triethylamine (0.8 g, 7.9 mmol) in ether (50 mL) added dropwise to the solution while 1-butyne was bubbled through the reaction mixture. The mixture was stirred at room temperature overnight, filtered, and the filtrate evaporated to dryness under reduced pressure. Recrystallisation of the residue from hexane gave the desired product (0.83 g, 90%) as a cream solid, melting point. 98-9° C.

出典